Characterization of Micro-Powders for the Fabrication of Compression Molded THz Lenses

We investigate different micro-powders that can be used as base materials for THz lenses fabricated by compression molding. For this application materials with a very weak THz absorbance and low dispersion are required. By measuring the THz absorption coefficient and refractive index of pellets pressed from the different micro-powders, we identify several materials that are well suited for the fabrication of compression molded THz lenses (CMLs). In addition, a considerable range of the refractive index is covered by the samples, which will allow for the fabrication of CMLs with different focal lengths for one and the same lens design.     

Optical reconstruction of high-speed surface dynamics in an uncontrollable environment

The ability to communicate with our voice can be regarded as the concatenation of the two processes "phonation" and "modulation." These take place in the larynx and palatal and oral region, respectively. During phonation the audible primary voice signal is created by mutual reaction of vocal folds with the exhaled air stream of the lungs. The underlying interactions of masses, fluids and acoustics have yet to be identified and understood. One part of the primary signal's acoustical source are vortex induced vibrations, as e.g., created by the Coand?effect in the air stream. The development of these vorteces is determined by the shape and 3-D movements of the vocal folds in the larynx. Current clinical in vivo research methods for vocal folds do not deliver data of satisfactory quality for fundamental research, e.g., an endoscope is limited to 2-D image information. Based hereupon, a few improved methods have been presented, however delivering only selective 3-D information, either for a single point or a line. This stands in contrast to the 3-D motions of the entire vocal fold surface. More complex imaging methods, such as MRI, do not deliver information in real-time. Thus, it is necessary to develop an easily applicable, more improved examination method, which allows for 3-D data of the vocal folds surfaces to be obtained. We present a method to calibrate a 3-D reconstruction setup including a laser projection system and a high-speed camera. The setup is designed with miniaturization and an in vivo application in mind. The laser projection system generates a divergent grid of 196 laser dots by diffraction gratings. It is calibrated with a planar calibration target through planar homography. In general, the setup allows to reconstruct the topology of a surface at high frame rates (up to 4000 frames per second) and in uncontrollable environments, as e.g., given by the lighting situation (little to no ambient light) and varying texture (e.g., varying grade of reflection) in the human larynx. In particular, this system measures the 3-D vocal fold surface dynamics during phonation. Applied to synthetic data, the calibration is shown to be robust (error approximately 0.5 μm) regarding noise and systematic errors. Experimental data gained with a linear z -stage proved that the system reconstructs the 3-D coordinates of points with an error at approximately 15 μm. The method was applied exemplarily to reconstruct porcine and artificial vocal folds' surfaces during phonation. Local differences such as asymmetry between left and right fold dynamics, as well as global parameters, such as opening and closing speed and maximum displacements, were identified and quantified.     

Compound-specific chlorine isotope analysis: a comparison of gas chromatography/isotope ratio mass spectrometry and gas chromatography/quadrupole mass spectrometry methods in an interlaboratory study

Chlorine isotope analysis of chlorinated hydrocarbons like trichloroethylene (TCE) is of emerging demand because these species are important environmental pollutants. Continuous flow analysis of noncombusted TCE molecules, either by gas chromatography/isotope ratio mass spectrometry (GC/IRMS) or by GC/quadrupole mass spectrometry (GC/qMS), was recently brought forward as innovative analytical solution. Despite early implementations, a benchmark for routine applications has been missing. This study systematically compared the performance of GC/qMS versus GC/IRMS in six laboratories involving eight different instruments (GC/IRMS, Isoprime and Thermo MAT-253; GC/qMS, Agilent 5973N, two Agilent 5975C, two Thermo DSQII, and one Thermo DSQI). Calibrations of (37)Cl/(35)Cl instrument data against the international SMOC scale (Standard Mean Ocean Chloride) deviated between instruments and over time. Therefore, at least two calibration standards are required to obtain true differences between samples. Amount dependency of δ(37)Cl was pronounced for some instruments, but could be eliminated by corrections, or by adjusting amplitudes of standards and samples. Precision decreased in the order GC/IRMS (1σ ≈ 0.1‰), to GC/qMS (1σ ≈ 0.2-0.5‰ for Agilent GC/qMS and 1σ ≈ 0.2-0.9‰ for Thermo GC/qMS). Nonetheless, δ(37)Cl values between laboratories showed good agreement when the same external standards were used. These results lend confidence to the methods and may serve as a benchmark for future applications.     

Polymers containing formamidine groups

Summary Aliphatic polyformamidines have been synthesized by reaction of aliphatic diamines with triethyl orthoformate in presence of catalytic amounts of acetic acid. The reaction has been carried out in DMSO at 180°C. The polymer structure has been confirmed by IR and NMR spectroscopy. For determination of molecular weights ¹H NMR end group signals have been used.     

Enol cation radicals in solution. 4. An improved Synthesis of 4,6,7-Trimethylbenzofurans by oxidation of β-mesityl substituted enols

An improved synthetic access for the construction of 4,6,7-trimethylbenzofurans ( B1–B8 ) through the one-electron oxidation of mesityl-substituted enols ( E1–E8 ) is presented. The transformation can be accomplished in good to excellent yields by using various oxidants; i.e. tris(1,10-phenanthroline)iron(III) hexafluorophosphate, FeCl₃, Ce(NH₄)₂(NO₃)₆, Cu(OTf)₂/Cu₂O or anodic oxidation.     

Reduction of Sulfoxides to Sulfides in the Presence of Copper Catalysts

Abstract  

Copper complexes catalyze the reduction of aliphatic and aromatic sulfoxides in the presence of silanes as reducing reagent. The influence of different reaction parameters on the catalytic activity is investigated in detail. The scope and limitations of the described catalyst is demonstrated in the reduction of various sulfoxides. In most cases, high conversion and excellent chemoselectivity are obtained.